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Method for preparing tert-butyl hydroperoxide employing biomimetic catalysis and isobutane oxidation

A technology of tert-butyl hydroperoxide and biomimetic catalysis of isobutane, which is applied to the preparation of peroxygen compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of poor selectivity of tert-butyl hydroperoxide and achieve The effect of avoiding environmental and safety problems, simple operation process, and good industrial application prospects

Active Publication Date: 2015-01-07
HUIZHOU RES INST OF SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

U.S. Patent US 405959 discloses a process for the preparation of propylene oxide by non-catalytic oxidation of isobutane-propylene epoxidation. This process needs to be operated under high temperature and pressure. Due to the high temperature decomposition of tert-butyl hydroperoxide, the selectivity of tert-butyl hydroperoxide is poor
In addition, U.S. Patents US4408082, US 3478108, US 3855314 and US 390720 disclose the use of methods higher than the critical condition of isobutane or adding a small amount of peroxide as an initiator to improve the conversion rate of isobutane and the selection of tert-butyl hydroperoxide resistance, but requires high temperature and pressure

Method used

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  • Method for preparing tert-butyl hydroperoxide employing biomimetic catalysis and isobutane oxidation
  • Method for preparing tert-butyl hydroperoxide employing biomimetic catalysis and isobutane oxidation
  • Method for preparing tert-butyl hydroperoxide employing biomimetic catalysis and isobutane oxidation

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Experimental program
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Effect test

Embodiment 1

[0021] In 100mL polytetrafluoroethylene-lined stainless steel reactor, add 20mL containing 100ppm metalloporphyrin (M 1 =Mn,X=H,R 1 =R 2 =R 3 =R 4 =R 5 =H) in 1,2-dichloroethane solution, filled with 10mol, filled with oxygen, the reaction pressure was 0.3MPa, stirred at a temperature of 40°C, and reacted for 7h, detected by gas chromatography, isobutyl The conversion of alkanes was 17%, and the selectivity to tert-butyl hydroperoxide was 99%.

Embodiment 2

[0023] In 100mL polytetrafluoroethylene-lined stainless steel reactor, add 30mL containing 0.1ppm metalloporphyrin (M 1 =Co,X=H,R 1 = NO 2 , R 2 =R 3 =R 4 =R 5 =H) in the 1,2-dichloroethane solution, filled with 20mmol of isobutane, filled with oxygen, the reaction pressure was 3MPa, stirred at a temperature of 100°C, reacted for 7h, analyzed by gas chromatography , the conversion of isobutane was 15%, and the selectivity of tert-butyl hydroperoxide was 91%.

Embodiment 3

[0025] Add 30mL containing 10ppm metalloporphyrin (M 2 =Fe,X=F,R 1 =R 2 =R 3 =R 4 =R 5 =H,X 1 Pyridine) in the acetonitrile solution, filled with 20mmol isobutane, filled with oxygen, the reaction pressure is 2MPa, stirred at a temperature of 60 ° C, after 7 hours of reaction, through gas chromatography analysis, the conversion rate of isobutane was 25 %, the selectivity of tert-butyl hydroperoxide is 95%.

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Abstract

The invention discloses a method for preparing tert-butyl hydroperoxide employing biomimetic catalysis and isobutane oxidation. According to the method, with isobutene as a raw material, oxygen as an oxidant, and a metal porphyrin compound as a catalyst, under the condition of controlling the reaction temperature at 40-100 DEG C and the reaction pressure at 0.3-3.0MPa, catalytic reaction is carried out to obtain the tert-butyl hydroperoxide. Compared with other processes, the method disclosed by the invention has the advantages of being mild in reaction condition, good in catalytic effect, high in tert-butyl hydroperoxide selectivity, simple in process and the like.

Description

technical field [0001] The invention relates to a method for preparing tert-butyl hydroperoxide, in particular to a method for preparing tert-butyl hydroperoxide by biomimetic catalysis of isobutane oxidation. Background technique [0002] As a kind of alkyl hydroperoxide, tert-butyl hydroperoxide is widely used as olefin polymerization initiator, polyester resin curing agent, oxidant, diesel oil cetane number improver and can be decomposed by itself to prepare tert-butanol and methanol and solvents such as acetone. [0003] Due to the wide application and high added value of tert-butyl hydroperoxide, its synthesis method has attracted extensive attention of researchers at home and abroad. At present, the methods for industrially synthesizing tert-butyl hydroperoxide mainly include: [0004] (1) sulfuric acid hydrogen peroxide method. The sulfuric acid hydrogen peroxide method uses isobutylene or tert-butanol as raw material, and a large amount of waste sulfuric acid is p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/04C07C407/00B01J31/22
Inventor 纪红兵周贤太曾超
Owner HUIZHOU RES INST OF SUN YAT SEN UNIV
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